CN115342910A - High-strength titanium alloy metallographic sample preparation method - Google Patents
High-strength titanium alloy metallographic sample preparation method Download PDFInfo
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- CN115342910A CN115342910A CN202210982070.6A CN202210982070A CN115342910A CN 115342910 A CN115342910 A CN 115342910A CN 202210982070 A CN202210982070 A CN 202210982070A CN 115342910 A CN115342910 A CN 115342910A
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 24
- 238000005464 sample preparation method Methods 0.000 title claims abstract description 13
- 238000005498 polishing Methods 0.000 claims abstract description 44
- 238000000227 grinding Methods 0.000 claims abstract description 28
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 10
- 239000010432 diamond Substances 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 239000003518 caustics Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 244000137852 Petrea volubilis Species 0.000 claims abstract description 3
- 238000000861 blow drying Methods 0.000 claims abstract description 3
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 17
- 239000004744 fabric Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 229910001040 Beta-titanium Inorganic materials 0.000 abstract description 12
- 229910045601 alloy Inorganic materials 0.000 abstract description 12
- 239000000956 alloy Substances 0.000 abstract description 12
- 238000005260 corrosion Methods 0.000 abstract description 8
- 230000007797 corrosion Effects 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- 230000003321 amplification Effects 0.000 description 6
- 238000003199 nucleic acid amplification method Methods 0.000 description 6
- 238000007517 polishing process Methods 0.000 description 6
- 239000000314 lubricant Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J1/00—Photometry, e.g. photographic exposure meter
- G01J1/02—Details
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a high-strength titanium alloy metallographic sample preparation method, which comprises the following steps: processing a sample to be detected into a test surface and embedding a metallographic phase; grinding the test surface on a grinding and polishing machine by using sand paper; polishing the ground test surface by a diamond polishing agent; and wiping the polished test surface by using a mixed corrosive agent, cleaning by using absolute ethyl alcohol, and blow-drying to obtain the required metallographic sample. The invention has the following beneficial effects: the high-strength titanium alloy metallographic sample preparation method provided by the invention is simple to operate, solves the problem that metallographic corrosion cannot clearly display the metallographic structure due to the fact that scratches and orange peel occur in the sample preparation process of similar near-beta titanium alloys such as Ti-1500, and can obtain a near-beta titanium alloy metallographic sample with a clear tissue structure and without scratches.
Description
Technical Field
The invention belongs to the field of metal microstructure determination, and particularly relates to a high-strength titanium alloy metallographic sample preparation method.
Background
With the rapid development of aerospace technology, various fastener parts of aircrafts have higher and higher requirements on high-strength titanium alloy, so that the high-strength and high-toughness titanium alloy with the tensile strength exceeding 1500MPa becomes a very important development direction. Titanium alloys can be classified into alpha titanium alloys, near-alpha titanium alloys, alpha + beta titanium alloys, near-beta titanium alloys, and beta titanium alloys according to the equilibrium structure of the titanium alloys at room temperature. Due to good toughness of the Ti-1500 near-beta titanium alloy, when a metallographic specimen is prepared, an orange peel phenomenon often appears on a detection surface of a polished specimen, as shown in figures 11-12, and a microstructure after corrosion cannot be clearly shown, as shown in figures 13-14.
Summary of the invention
In view of this, the invention aims to provide a metallographic sample preparation method for a high-strength titanium alloy, so as to avoid the phenomenon of orange peel and enable a microstructure to clearly display metallographic corrosion.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a metallographic sample preparation method for a high-strength titanium alloy comprises the following steps:
s1: processing a sample to be detected into a test surface and embedding a metallographic phase; preferably, the fastener made of the Ti-1500 material is cut into sections through wire cutting to form a test surface, and then the test surface is inlaid through a transparent metallographic inlaid material, so that no gap is formed between the surface of the sample and the inlaid material, and the pollution of the test surface of the sample caused by no acid leaching in the corrosion process is avoided;
s2: grinding the test surface on a grinding and polishing machine by using sand paper;
s3: polishing the ground test surface by a diamond polishing agent until fine scratches and orange peel can be removed;
s4: and wiping the polished test surface by using a mixed corrosive agent, cleaning by using absolute ethyl alcohol, and blow-drying to obtain the required clean and scratch-free metallographic specimen.
Furthermore, in step S2, the 120# sandpaper, the 600# sandpaper and the 2000# sandpaper are sequentially used for grinding, the rotation speed of the grinding and polishing disc is 200rpm, the grinding pressure is 1.8daN, the rotation speed of the clamp is 120rpm, and the rotation directions of the grinding and polishing disc and the clamp are the same.
Further, the sanding time of No. 120 sandpaper was 250s, the sanding time of No. 600 sandpaper was 180s, and the sanding time of No. 2000 sandpaper was 120s.
Further, in step S3, velvet is used as polishing cloth, and diamond polishing agent of 3.5 μm and 0.5 μm is sequentially polished, the rotation speed of the polishing cloth is 200rpm, the polishing pressure is 1.8daN, the rotation speed of the clamp is 120rpm, and the rotation directions of the polishing cloth and the clamp are the same.
Further, the mixed corrosive comprises the following components in parts by volume: 2 parts of hydrofluoric acid, 3 parts of hydrochloric acid, 5 parts of nitric acid and 190 parts of water.
Further, the mixed etchant wiping time is 30-120s.
Compared with the prior art, the high-strength titanium alloy metallographic sample preparation method provided by the invention has the following advantages:
the high-strength titanium alloy metallographic sample preparation method provided by the invention is simple to operate, solves the problem that metallographic corrosion cannot clearly display the metallographic structure due to the fact that scratches and orange peel occur in the sample preparation process of similar near-beta titanium alloys such as Ti-1500, and can obtain a near-beta titanium alloy metallographic sample with a clear tissue structure and without scratches.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and, together with the description, serve to explain the invention without limitation. In the drawings:
FIG. 1 is a schematic 50-fold enlarged view of a test surface of a polished sample of inventive example 1;
FIG. 2 is a schematic view at 500 times magnification of a test surface of a polished sample of inventive example 1;
FIG. 3 is a schematic view of a test surface of a sample after etching at a magnification of 200 times in inventive example 1;
FIG. 4 is a schematic view at 500 times magnification of a test surface of a sample after corrosion according to inventive example 1;
FIG. 5 is a schematic enlarged 100 times of a test surface of a polished sample of comparative example 1 created by the present invention;
FIG. 6 is a schematic enlarged 200 times of a test surface of a polished sample of comparative example 1 according to the invention;
FIG. 7 is a schematic view at 500 times magnification of a test surface of a polished sample of comparative example 1 created by the present invention;
FIG. 8 is a schematic 100-fold enlarged view of a test surface of a polished sample of inventive comparative example 2;
FIG. 9 is a schematic enlarged 200 times of a test surface of a polished sample of comparative example 2 created by the present invention;
FIG. 10 is a schematic view at 500 times magnification of a test surface of a polished sample of comparative example 2 created by the present invention;
FIG. 11 is a schematic view showing a phenomenon of "orange peel" appearing on a test surface of a Ti-1500 near-beta titanium alloy after polishing in the prior art;
FIG. 12 is a schematic view showing the appearance of "orange peel" on a test surface of a Ti-1500 near-beta titanium alloy after polishing in the prior art;
FIG. 13 is an enlarged schematic view of a test surface of a prior art sample after corrosion of a Ti-1500 near-beta titanium alloy;
FIG. 14 is an enlarged view of a test surface of a prior art sample after corrosion of a Ti-1500 near-beta titanium alloy.
Detailed Description
It should be noted that the embodiments and features of the embodiments of the present invention may be combined with each other without conflict.
The invention will be described in detail with reference to the following embodiments with reference to the attached drawings.
The high-strength titanium alloy metallographic sample preparation method in the embodiment comprises the following steps:
s1: cutting the fastener made of the Ti-1500 material through wire cutting to form a test surface, and embedding the test surface through a transparent metallographic embedding material to ensure that no gap exists between the surface of the sample and the embedding material;
s2: grinding the test surface by using 120# abrasive paper, 600# abrasive paper and 2000# abrasive paper on a grinding and polishing machine in sequence, wherein the grinding process parameters are shown in table 1;
| serial number | 1 | 2 | 3 |
| Grinding and polishing disk | 120# abrasive paper | 600# abrasive paper | 2000# abrasive paper |
| Rotational speed (rpm) | 200 | 200 | 200 |
| Lubricant agent | Water (W) | Water (I) | Water (W) |
| Force (daN) | 1.8 | 1.8 | 1.8 |
| Clamp rotating speed (rpm) | 120 | 120 | 120 |
| Direction of rotation | In the same direction | In the same direction | In the same direction |
| Time(s) | 250s | 180s | 120s |
TABLE 1 grinding Process parameters
S3: polishing the ground test surface by using velvet as polishing cloth and sequentially using diamond polishing agents with the particle sizes of 3.5 micrometers and 0.5 micrometer, wherein the polishing process parameters are shown in table 2 until fine scratches and orange peel can be removed, the polished test surface is magnified by 50 times as shown in figure 1, and is magnified by 500 times as shown in figure 2;
TABLE 2 polishing Process parameters
S4: wiping the polished test surface by using a mixed corrosive, wherein the mixed corrosive comprises the following components in parts by volume: 2 parts of hydrofluoric acid, 3 parts of hydrochloric acid, 5 parts of nitric acid and 190 parts of water, wherein the wiping time of the mixed corrosive agent is 30-120s, then the mixed corrosive agent is cleaned by absolute ethyl alcohol and dried by blowing, and a clean and scratch-free metallographic specimen is obtained, wherein the magnification is 200 times as shown in figure 3, and the magnification is 500 times as shown in figure 4.
Comparative example 1
The high-strength titanium alloy metallographic phase sample preparation method in the comparative example comprises the following steps:
s1: cutting the fastener made of the Ti-1500 material through wire cutting to form a test surface, and embedding the test surface through a transparent metallographic embedding material to ensure that no gap exists between the surface of the sample and the embedding material;
s2: grinding the test surface by using 120# abrasive paper, 600# abrasive paper and 2000# abrasive paper on a grinding and polishing machine in sequence, wherein the grinding process parameters are shown in table 3;
| serial number | 1 | 2 | 3 |
| Grinding and polishing disk | 120# abrasive paper | 600# abrasive paper | 2000# abrasive paper |
| Rotational speed (rpm) | 150 | 150 | 150 |
| Lubricant agent | Water (W) | Water (W) | Water (W) |
| Force (daN) | 1.5 | 1.5 | 1.5 |
| Clamp rotating speed (rpm) | 80 | 80 | 80 |
| Direction of rotation | In the same direction | In the same direction | In the same direction |
| Time(s) | 100s | 180s | 180s |
TABLE 3 grinding Process parameters
S3: polishing the ground test surface by using a diamond polishing agent with the particle size of 3.5 microns by using velvet as polishing cloth, wherein the polishing process parameters are shown in table 4, the amplification of the polished test surface is 100 times as shown in fig. 5, the amplification of the test surface is 200 times as shown in fig. 6, and the amplification of the test surface is 500 times as shown in fig. 7;
| step (ii) of | 4 |
| Polishing cloth | Polishing cloth |
| Rotational speed (rpm) | 150 |
| Lubricant agent | 3.5 μm diamond |
| Force (daN) | 1.5 |
| Clamp rotating speed (rpm) | 80 |
| Direction of rotation | In the same direction |
| Time(s) | 180s |
TABLE 4 polishing Process parameters
As can be seen from fig. 5 to 7, the metallographic specimen prepared in this comparative example had a large number of scratches on the surface thereof, and the structure of the metallographic specimen could not be clearly observed.
Comparative example 2
The high-strength titanium alloy metallographic phase sample preparation method in the comparative example comprises the following steps:
s1: cutting the fastener made of the Ti-1500 material through wire cutting to form a test surface, and embedding the test surface through a transparent metallographic embedding material to ensure that no gap exists between the surface of the sample and the embedding material;
s2: grinding the test surface by using 120# abrasive paper, 600# abrasive paper and 2000# abrasive paper on a grinding and polishing machine in sequence, wherein the grinding process parameters are shown in table 5;
TABLE 5 grinding Process parameters
S3: polishing the ground test surface by using a diamond polishing agent with the particle size of 3.5 microns by using velvet as polishing cloth, wherein the polishing process parameters are shown in table 6, the amplification of the polished test surface is 100 times as shown in fig. 8, the amplification of the test surface is 200 times as shown in fig. 9, and the amplification of the test surface is 500 times as shown in fig. 10;
| step (ii) of | 4 |
| Polishing cloth | Polishing cloth |
| Rotational speed (rpm) | 200 |
| Lubricant agent | 3.5 μm diamond |
| Force (daN) | 1.8 |
| Clamp rotating speed (rpm) | 120 |
| Direction of rotation | In the same direction |
| Time(s) | 120s |
TABLE 6 polishing Process parameters
As can be seen from fig. 8 to 10, the metallographic specimen prepared in this comparative example had many fine scratches on the surface thereof, and the structure of the metallographic specimen could not be clearly observed.
Claims (6)
1. A high-strength titanium alloy metallographic sample preparation method is characterized by comprising the following steps:
s1: processing a sample to be detected into a test surface and embedding a metallographic phase;
s2: grinding the test surface on a grinding and polishing machine by using sand paper;
s3: polishing the ground test surface by a diamond polishing agent;
s4: and wiping the polished test surface by using a mixed corrosive agent, cleaning by using absolute ethyl alcohol, and blow-drying to obtain the required metallographic sample.
2. The method for preparing the metallographic phase of the high-strength titanium alloy according to claim 1, wherein the method comprises the following steps: and step S2, grinding by using 120# abrasive paper, 600# abrasive paper and 2000# abrasive paper in sequence, wherein the rotation speed of the grinding and polishing disc is 200rpm, the grinding pressure is 1.8daN, the rotation speed of the clamp is 120rpm, and the rotation directions of the grinding and polishing disc and the clamp are the same.
3. The method for preparing the metallographic phase of the high-strength titanium alloy according to claim 2, wherein the method comprises the following steps: the sanding time of No. 120 sandpaper was 250s, the sanding time of No. 600 sandpaper was 180s, and the sanding time of No. 2000 sandpaper was 120s.
4. The method for preparing the metallographic phase of the high-strength titanium alloy according to claim 1, wherein the method comprises the following steps: and step S3, polishing by using velvet as polishing cloth and sequentially using diamond polishing agents with the particle size of 3.5 microns and 0.5 micron, wherein the rotating speed of the polishing cloth is 200rpm, the polishing pressure is 1.8daN, the rotating speed of the clamp is 120rpm, and the rotating directions of the polishing cloth and the clamp are the same.
5. The method for preparing the metallographic phase of the high-strength titanium alloy according to claim 1, wherein the method comprises the following steps: the mixed corrosive comprises the following components in parts by volume: 2 parts of hydrofluoric acid, 3 parts of hydrochloric acid, 5 parts of nitric acid and 190 parts of water.
6. The method for preparing the metallographic phase of the high-strength titanium alloy according to claim 1, wherein the method comprises the following steps: the mixed etchant has a wiping time of 30-120s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210982070.6A CN115342910A (en) | 2022-08-16 | 2022-08-16 | High-strength titanium alloy metallographic sample preparation method |
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|---|---|---|---|
| CN202210982070.6A CN115342910A (en) | 2022-08-16 | 2022-08-16 | High-strength titanium alloy metallographic sample preparation method |
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| CN115342910A true CN115342910A (en) | 2022-11-15 |
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|---|---|---|---|
| CN202210982070.6A Pending CN115342910A (en) | 2022-08-16 | 2022-08-16 | High-strength titanium alloy metallographic sample preparation method |
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